反应详情

温度

90 °C

To a 3000 mL round bottom flask, 3-bromoaniline (50 g, 0.2907 mol), water (1500 mL), chloral hydrate (57.7 g, 0.3488 mol), hydroxylamine hydrochloride (64.6 g, 0.9302 mol) and sodium sulphate (250 g) were added. To this reaction mixture was slowly added concentrated HCl (76 mL). The reaction mixture was stirred at 90° C. for 2 hours. The white precipitate was formed and was collected by filtration. The white solid was dried to provide the title compound [60 g, 85%]. 1H NMR (300 MHz, DMSO-d6): δ 12.28 (s, 1H), 10.38 (s, 1H), 8.03 (t, J=1.5 Hz, 1H), 7.62-7.65 (m, 2H), 7.29-7.31 (m, 2H). LC-MS (ESI): Calculated mass: 242.0; Observed mass [M+H]+: 243.0 (RT: 0.17 min).

1. customThe white precipitate was formed
2. filtrationwas collected by filtration
3. customThe white solid was dried